corrosion concerns and testing for electronic...

University of MarylandCopyright © 2015 CALCE

1Center for Advanced Life Cycle Engineeringwww.calce.umd.edu Innovation Award Winner

Corrosion Concerns and Testing for Electronic Equipment

Michael [email protected] of MarylandCollege Park, MD 20742

iNEMI Research Webinar SeriesApril 30, 2015



What is CALCE?Center for Advanced Life Cycle Engineering (founded 1987) is dedicated to providing a knowledge and resource base to support the development and sustainment of competitive electronic components, products and systems. Focus areas:

• Physics of Failure • Design of Reliability• Accelerated Qualification• Supply-chain Management• Obsolescence• Prognostics

Center Organization

16 research faculty 5 technical staff 40+ PhD students20+ MS students11 visiting scholars

http://www.calce.umd.edu

CALCECenter for Advanced Life Cycle Engineering

forElectronic Products

and Systems

Research Contracts

• Large scale programs • Medium to long‐term durations• Contractual agreements• Examples:

Software development,testing, training programs

Electronic Products

and SystemsConsortium

•Risk assessment, management, and mitigation for electronics

Prognostics and Health ManagementConsortium

• Techniques based on data trending, physics‐of‐failure, and fusion

Education

• MS and PhD programs• International visitors• Web seminars • Short courses for industry

LabServices

• Small to medium scale• Rapid response• Examples: Failure analysis, measurement,design review, supplier assessment

Standards• Putting CALCE research to work for industry

• Examples:IEEE GEIA IPCJEDECIEC



• High atmospheric concentrations of sulfur can be found in a wide variety of industries that use electronics [1]• Pulp and paper industry (by-product of wood degradation)• Sewage treatment (by-product of organic degradation)• Construction (released during excavation)• Iron smelting (by-product of smelting process)• Mining (found in mineral rock)

Corrosive Sulfur Environments

1. “Hydrogen Sulfide in Industry”. WorkSafeBC website. Workers' Compensation Board of British Columbia. (2007)



Corrosion on Fielded Electronic Systems

• Corrosion of silver in a fielded resistor array

• Corrosion on a PCB in a clay modeling facility for a month and a half [1]

• ENIG-plated connectors corroded during shipping and handling

[1] Mazurkiewicz, P., “Accelerated corrosion of PCBs due to high levels of reduced sulfur gasses in industrial environments,” Proceedings of the 32nd International Symposium for Testing and Failure Analysis, Austin, TX, 2006



Corrosion of Electronic Systems• Different chemistries (Sulfides, Chlorides, etc.) can attack

metals used in electronic systems (Cu, Ag, Ni, etc.)• Heat and moisture can increase reactivity• Reactive materials can be a result of improper cleanliness

or a corrosive environment (Shipping, Storage or Use)

Corrosive Environment

Moisture

Reactive Chemicals

HeatPre-Exposure Post-Exposure

Copper coupons are commonly used as witness coupons for measuring corrosive environments

[1] Rice et al. Atmospheric Corrosion of Copper and Silver. Journal of the Electrochemical Society 128.2. (1981)

[1]



Corrosion vs. Electrochemical MigrationCorrosion Electrochemical

Migration

Copper (+)

Copper (-)

+- e-

Cu2+ H20Dendrite

Coppere- Cu+ Cu2+

H20

• Driven by an electrical potential in the presence of water

• Leads to the formation of metal dendrites

Corrosive Gases(SO2, Cl2, H2S)

• Driven by the oxidation of metal

• Does not require water• Formation of corrosion

products (not pure Metal)

Corrosion Products(Cu2O, CuCl, Cu2S…)

Acids and Ions



Classification of Corrosive Environment• Corrosivity of an environment for electronics is often

characterized by copper corrosion film thickness.• There are various methods that can be used to measure film

thickness, each with their advantages and disadvantages.

BattelleSeverity

Class1 year

film thicknessI <35 nmII 40 to 70 nmIII 80 to 400 nmIV >500 nm

Classifying environments using copper coupons. [1]

• Pro: Simple method• Con: Bad assumption of products

Weight Gain

• Pro: Does not require pre- exposure data• Con: Underestimates corrosion

Cathodic Reduction

• Pro: Accurate measurement• Cons: Requires ion milling

Profilometry



ASHRAE - 2011 Gaseous and Particulate Contamination Guidelines For Data Centers

• Airborne Particles • Mechanical, Chemical, and Electrical effects• Recommendation that data centers be kept clean to ISO Class 8• Restricting particle size is thought to reduce harmful dust (with

high ionic contamination)• Gaseous contamination

• ISA -71.04 Gaseous Corrosivity level of G1• Reactivity monitoring recommended

• Maximum corrosion rate of copper should be <200 Å/month• Maximum corrosion rate of silver should be <200 Å/month

• Gas filtration can be used to meet these goals



Corrosion Testing of Electronics

Humidity Thermal Storage Salt Spray

Mixed Flowing Gas

Flowers of Sulfur Clay



Mixed Flowing Gas Testing

MFG chamber used at CALCESchematic for a MFG chamber

• Mixed flowing gas testing uses corrosive gases, heaters, and humidifiers to provide an accelerated corrosion test environment

• Different standards provide chamber conditions that can be used to reach target corrosion levels (i.e. ASTM B827 (Practice) and ASTM B845 (Electrical contacts))



Standards for MFG Testing

Battelle• Environmental classification from least(Class I) to most(Class IV)• Classes II-IV have accelerated test conditions: 2 days in chamber = 1 year in field

EIA• Environmental classification from least(Class I) to most(Class IV)• Class IIA-IV is an accelerated test conditions: 5 days in chamber = 3 years in field

IEC• Method 1 is for gold coatings• Methods 2-4 are for electronics in moderate(2&4) and severe(3) environments

Telcordia• Test methods for telecommunication equipment in indoor and outdoor settings

IBM• G1(T) is accelerated test for a business office environment



Standards for MFG TestingCreator Class Temp (ºC) RH (%) H2S (ppb) Cl2 (ppb) NO2 (ppb) SO2 (ppb)

Battelle II 30±2 70±2 10+0/-4 10+0/-2 200±25 ---

III 30±2 75±2 100±10 20±5 200±25 ---

IV 50±2 75±2 200±10 50±5 200±25 ---

EIA-364-65 II 30±2 70±2 10±5 10±3 200±25 ---

IIA 30±1 70±2 10±5 10±3 200±25 100±20

III 30±2 75±2 100±20 20±5 200±25 ---

IIIA 30±1 70±2 100±20 20±5 200±25 200±50

IV 40±2 75±2 200±20 30±5 200±25 ---

IEC 68-2-60 1 25±1 75±3 100±20 --- --- 500±100

2 30±1 75±3 10±5 10±5 200±50 ---

3 30±1 75±3 100±20 20±5 200±50 ---

4 25±1 75±3 10±5 10±5 200±50 200±20

Telcordia GR-63-CORE 5.5

Indoor 30±1 70±2 10±1.5 10±1.5 200±30 100±15

Outdoor 30±1 70±2 100±15 20±3 200±30 200±30

IBM G1 30±.5 70±2 40±5% 3±15% 610±5% 350±5%



* Number in brackets indicates number of samples in test

Copper Coupon Weight Gain of MFG Test Environments



Flowers of Sulfur Test• The Flowers of Sulfur (FoS) test is described in ASTM-B809,

and uses a chamber with a sulfur source and a humidity source in an oven to create a corrosive test environment

• Variations of this test include high temperatures and no moisture

Samples

Sensor

Sealed Chamber Sulfur Source

Oven

Salt solutionSamples

Sulfur Source

Salt solution

FoS test chamber used at CALCESchematic for a FoS testing



Elevated Temperature and Duration Test PlanA series of tests were carried out in the ASTM test vessel

• Temperatures (°C): 50, 75, 85, 95 and 105• Durations (days): 1, 5, 10, and 15• Specimen: 3 copper coupons

SamplesSulfur source

Salt solution1 5 10 15

50758595105

Test Matrix

Tem

pera

ture

(ºC

)

Duration (Days)



FOS Data – Temperature PlotCopper Corrosion Thickness



P values 50 °C 75 °C 85 °C 95 °C 105 °C1 day 5 day 10 day 15 day 1 day 10 day 1 day 5 day 10 day 15 day 1 day 10 day 1 day 5 day 10 day

50 °C

1 day 3.28E‐01 2.01E‐01 8.28E‐02 1.04E‐01 9.37E‐04 4.17E‐04 6.42E‐03 5.04E‐06 8.49E‐06 3.37E‐03 9.08E‐04 1.05E‐04 5.18E‐06 2.90E‐045 day 3.28E‐01 3.40E‐01 1.36E‐01 2.04E‐01 9.82E‐04 9.21E‐03 7.12E‐03 5.46E‐06 8.54E‐06 5.60E‐03 9.16E‐04 2.17E‐04 5.61E‐06 2.92E‐0410 day 2.01E‐01 3.40E‐01 5.53E‐01 8.90E‐01 1.28E‐03 6.61E‐01 1.06E‐02 9.74E‐06 8.79E‐06 4.87E‐02 9.43E‐04 4.51E‐03 9.92E‐06 2.99E‐0415 day 8.28E‐02 1.36E‐01 5.53E‐01 6.02E‐01 1.41E‐03 6.82E‐01 1.36E‐02 1.12E‐05 8.92E‐06 1.19E‐01 9.62E‐04 9.78E‐03 1.14E‐05 3.04E‐04

75 °C 1 day 1.04E‐01 2.04E‐01 8.90E‐01 6.02E‐01 1.21E‐03 7.45E‐01 1.05E‐02 8.27E‐06 8.76E‐06 4.08E‐02 9.45E‐04 2.78E‐03 8.44E‐06 3.00E‐0410 day 9.37E‐04 9.82E‐04 1.28E‐03 1.41E‐03 1.21E‐03 X 1.07E‐03 1.45E‐02 3.84E‐02 3.24E‐04 1.56E‐03 1.41E‐02 1.78E‐03 3.74E‐02 5.23E‐03

85 °C

1 day 4.17E‐04 9.21E‐03 6.61E‐01 6.82E‐01 7.45E‐01 1.07E‐03 1.01E‐02 5.74E‐06 8.70E‐06 1.85E‐02 9.48E‐04 2.90E‐04 5.90E‐06 3.00E‐045 day 6.42E‐03 7.12E‐03 1.06E‐02 1.36E‐02 1.05E‐02 1.45E‐02 1.01E‐02 3.49E‐04 1.23E‐05 2.50E‐02 1.37E‐03 5.45E‐02 3.46E‐04 4.13E‐0410 day 5.04E‐06 5.46E‐06 9.74E‐06 1.12E‐05 8.27E‐06 3.84E‐02 5.74E‐06 3.49E‐04 1.96E‐05 1.06E‐05 3.86E‐03 1.04E‐05 9.43E‐01 9.28E‐0415 day 8.49E‐06 8.54E‐06 8.79E‐06 8.92E‐06 8.76E‐06 3.24E‐04 8.70E‐06 1.23E‐05 1.96E‐05 9.15E‐06 3.96E‐03 9.41E‐06 1.96E‐05 1.16E‐02

95 °C 1 day 3.37E‐03 5.60E‐03 4.87E‐02 1.19E‐01 4.08E‐02 1.56E‐03 1.85E‐02 2.50E‐02 1.06E‐05 9.15E‐06 1.02E‐03 4.14E‐02 1.08E‐05 3.18E‐0410 day 9.08E‐04 9.16E‐04 9.43E‐04 9.62E‐04 9.45E‐04 1.41E‐02 9.48E‐04 1.37E‐03 3.86E‐03 3.96E‐03 1.02E‐03 1.08E‐03 3.88E‐03 2.01E‐01

105 °C1 day 1.05E‐04 2.17E‐04 4.51E‐03 9.78E‐03 2.78E‐03 1.78E‐03 2.90E‐04 5.45E‐02 1.04E‐05 9.41E‐06 4.14E‐02 1.08E‐03 1.07E‐05 3.34E‐045 day 5.18E‐06 5.61E‐06 9.92E‐06 1.14E‐05 8.44E‐06 3.74E‐02 5.90E‐06 3.46E‐04 9.43E‐01 1.96E‐05 1.08E‐05 3.88E‐03 1.07E‐05 9.33E‐0410 day 2.90E‐04 2.92E‐04 2.99E‐04 3.04E‐04 3.00E‐04 5.23E‐03 3.00E‐04 4.13E‐04 9.28E‐04 1.16E‐02 3.18E‐04 2.01E‐01 3.34E‐04 9.33E‐04

• ANOVAs were performed to compare pairs of sample• F‐test used to compare variance between/within test groups• 90% probability was used (p‐value < 0.1 highlighted below)

• Assumed independent samples (different locations) and normal distribution of corrosion weight gain [1]

1. ASTM International. “Corrosion Tests and Standards”, ASTM, Baltimore, MD (2005)

P-values for F-testing between FOS test pairs

Analysis of Variance



Model Fitting to Averages

Θ = Corrosion Film Thickness (nm)X = Constant (nm) Y = Constant (1/ºC)Z = Constant (1/hoursX = 2.304 Y = 0.07057 Z = 0.01324 R2 = 0.9829

Θ Xe

Thi

ckne

ss (n

m)



Clay Testing• The Clay Test uses high sulfur modeling clay (30-50% elemental

sulfur) to create a sulfur-rich test environment• Heating wetted clay (45 - 55⁰C) releases sulfur• Samples placed in the test chamber may be cooled to increase

condensation onto the samples

Clay test using bulk clayClay test using shredded clay



Clay Test Weight Gain

• Ultra-Conductive Copper (Alloy 101)• Size of the Sample :-14mm*14mm• Thickness – 0.49mm• Number of Samples – 10• Hole Size: 2.55mm(Diameter)• Area =176.375mm2



Comparison of TestsCopper Weight Gain

This plot is based on copper weight gain. Coupons used for these measurements were ultra-pure copper with base weights between .65 to 0.9 grams



Comparison of 10-Day Test Environments

Test ConditionsWeight Gain(mg/g)

Thickness(nm/day)

Yrs in Class 4 Batelle Env.

H2S - 1800 ppb, 20% RH 0.08 113.7 2.3H2S - 250 ppb,75% RH 0.09 125.7 2.5H2S - 1800ppb, 75% RH 0.12 163.2 3.3FoS - 50C 0.40 542.3 10.84 gas - 200ppb/40C/75%RH 0.46 636.8 12.74 gas - 200ppb/40C/75%RH 0.49 677.1 13.54 gas - 200ppb/50C/50%RH 0.69 946.0 18.9FoS - 75C 0.76 1042.4 20.8FoS - 85C 1.47 2017.6 40.44 gas - 1700ppb/40C/75%RH 2.80 3838.5 76.8FoS - 105C 39.44 54094.2 1081.9

• Note: These calculations are based on composition assumptions for MFG testing. FOS product composition must be better understood.



Comparison of Corrosion Tests

Test Benefits WeaknessesMixed Flowing Gas

• Multiple Contaminants• Adjustable Concentrations• In-line Monitoring

• Limited Temperature Range

• Gases are expensive• Chamber has significant

maintenanceFlowersof Sulfur

• Salt Solution controls RH• Easily reusable chamber• Requires only a vessel, an

oven, and consumables

• Only sulfur contamination• Oven must be on for

entirety of test duration

Clay Test

• Only one consumable• Does not require an oven

• Only sulfur contamination• Periodic heating of clay



ENEPIG Test Vehicle (2011 Study)

Pads

Resistors

Resistors

UnpoweredComb Fingers

•ENEPIG Version #BNi: 4.53±0.15m Pd: 0.05±0.004mAu: 0.05±0.002m

•ENEPIG Version #CNi: 4.17±0.16m Pd: 0.154±0.006m Au: 0.04±0.003m

•ImAgAg: 0.33±0.06m

• Two Solders: SAC305 and SnPb• Observed Features – Optical Inspection

Six 2512 Resistors Three different pad sizes Eight comb finger structures

4 powered, 4 unpowered (5V bias with a11 kΩ resistor) 4 covered by BGA, 4 not covered by BGA(2 of each powered)

Forty pads (Four per resistor and four per chip)

PoweredComb Fingers



ENEPIG Test Matrix

ENEPIG ‐ B ENEPIG ‐ C ImAg

SnPb 1 1 1

SAC305 1 1 1

Solder TypeSurface Finish

Test ConditionsTemperature: 50oC Hydrogen Sulfide (H2S): 200 ppb Sulfur Dioxide (SO2): 200 ppbRelative Humidity: 75% Chlorine (Cl2): 50 ppb Nitrogen Dioxide (NO2): 200 ppb

These conditions represent a GX class exposure as there was more than 2000 nm/day of corrosion products.

Copper

Ag - Pure

Ag - Sterling

Average weight gain of 12 coupons



Optical Inspection – Pads• The exposure resulted in pad discoloration

Immersion Silver (2.5×)

ENEPIG B (2.5×)

ENEPIG C (2.5×)

Unexposed 5 day 10 day



Day 10 - Optical Inspection

Dendrite observed growing onENEPIG-C SnPb S2-Fingers 5-6 (Biased)

100x5x

20x



Inspection of Comb Fingers

Covered Comb Structure Exposed Comb Structure

Fingers completely covered with copper and sulfur

Corrosion spots composed of copper and sulfur detected



ENEPIG TestSurface Insulation Resistance measurement

• Resistance measurements of the comb structures were conducted prior to MFG exposure using a high resistance meter.

• They all showed a nominal resistance value of ~ 2 × 1010 Ω.• The failure criteria was a two order of magnitude drop in

resistance.• A 5 day exposure resulted in the failure of two structures that

were uncovered and under bias in ENEPIG Version B – SAC305. • A 10 day exposure resulted in additional failures.

E-B-SnPb E-B-SAC305 E-C-SnPb E-C-SAC305 ISA-SnPb ISA-SAC305Biased‐Uncovered 0 4 3 4 0 0Biased-Covered 0 1 1 0 0 0Unbiased–Covered 0 1 0 0 0 0Unbiased-Uncovered 0 2 0 0 0 0

# of failed samples on day 10 (four comb structures in each test group)



Corrosion Testing: Leadframes

Telcordia Outdoor – 10 Days Batelle III – 240 hours

• Several MFG test environments were used to generate corrosion on noble metal leadframes

• Only Telcordia Indoor conditions failed to generate corrosion



Examination of Coating On Creep CorrosionPart

• CY37128P100-125axi• Pitch 0.28• Plating Ni/Pd/Au• Lead wire: Copper Alloy

Coatings• Acrylic (AR): Type 1 (machine spray)

and Type 2 (hand spray)• Silicone (SR) by machine spray• Polyurethane (UR) by machine spray• Parylene (XY) by vacuum deposition• ALD-Cap O5TA200* by vacuum

deposition



Test Condition• Coated and non-coated test specimens were separated into two

groups to be subjected to environmental loading sequences.– TC: Temperature cycling for 100 cycles with 30 min dwells

Cycle A (-55°C/20°C) / Cycle B (-15°C/60°C) / Cycle C (20°C/95°C)– TH: Temperature Humidity with 50°C/50% RH for 200 hrs– Mixed Flowing Gases (MFG) for 48 hrs (EIA-364-TP65A class IV)

• Accumulated Loading Cycles

• Inspections of all components for tin whisker growth are conducted after each accumulated loading cycle with TC, TH, and MFG by optical and scanning electron microscopes.

TC-A TC-B TC-C MFG TH

Class Temp (°C) RH (%) H2S (ppb) Cl2 (ppb) NO2 (ppb) SO2 (ppb)

IV 50 ± 2 75 ± 2 200 ± 20 30 ± 5 200 ± 50 200 ± 50



Creep Corrosion on TQFPs

Non-coated AR1 XY

• With the exception of Parylene C, corrosion products were observed on the surfaces of all Ni/Pd/Au finished TQFP leads which were subject to MFG exposure.

WithoutMFG

With MFG

After 3rd Load Cycle



Acrylic Coatings

AR2

For the acrylic coatings, corrosion products were restricted to the edge of the terminals where coating coverage was thin or non-existent. Here, AR1 performed better than AR2. This result may be due to the differences in coverage. An examination of coverage is under way.

AR1



Silicone and Urethane Results

SR URSilicone showed substantial damage while UR was restricted to edges that had little to no coverage.



Parylene and ALD Results

ALD

Other than areas that had damage prior test, the Parylene coated specimens show no corrosion damage. The ALD coating showed corrosion on all terminals.

XY



Creep Corrosion on TQFPs• Cu whiskers and dendrites were observed on the corroded surface of

TQFPs with MFG exposure on non-coated and AR1, AR2, SR, UR and ALD coating.

• The sulfur (S) and chlorine (Cl) were detected via EDX on the corroded surfaces.

• Only Parylene C coated specimens were free from corrosion and no whiskers or dendrites were observed.

AR1 ALDSR



Creep Corrosion on TQFPsNon-Coated

SR

AR1

ALDAR2

UR



EDX Mapping ResultS Cl

Cu

Creep Corrosionon Non-coated TQFPs



Background on Thin Film Chip Resistors• Surface mount thick film chip resistors are inexpensive parts used in a

variety of electronic systems• The silver layer of chip resistors corrodes in sulfur-containing

environments, forming silver sulfide

Overcoat

Ceramic Substrate

Inner Ag

Resistor Element

OvercoatSolder Termination

Protective Barrier

Solder Termination

Ceramic Substrate



Comparison of Overlap Between Overcoat and Metallization

Type 1 2 3

4 5 6

Coat

Inner Electrode

Termination

Substrate



Corrosion Testing: Chip Resistors• Flowers of Sulfur Testing carried at 85°C (30 days)

– Formation of silver sulfide [failure in damaged resistors]

Ag2S

Before(As-received)

After(As-received)

Ag2S

ExposedAg

Before(Damaged)

After(Damaged)



Maximum Stress SnPb v/s SAC

Solder Max., Stress

SnPb 62 MPa

SAC305 83 MPa

Board 1.57 mmCopper 70 µm

Nickel 20 µm

Standoff 63.5 µm

Silver 10 µm

Alumina 550 µm

Element 20 µm

Coat 10 µm



Torsional Loads on Sample DIMM Cards• Torsional loading imposes cyclic out-of-plane deformation to a populated PCBA.• A portion of this deformation is transferred to the interface between interface of

overcoat and metallization in proportion to stiffness of board, rigidity of electronic components, compliance of leads and the solder interconnects.

Ang

le o

f tw

ist

Time

184 Pin DDR DIMM CardDDR – Double data rateDIMM – Dual in-line memory module

R-Net



Test MethodologyDDR 256MB DIMM 184-pin

Torsion Test ±18° 2000 cyc.

R-Net Visual Inspection

Control Set

105°C/24Hr FoS Exposure

R-Net Visual Inspection

• Torque 15 in-lb• Velocity 40°/sec• Hold time: 1 sec at +/- extremes



Photo Documentation

Post FoS test

Post torsion and FoS

Con

trol

Gro

upTo

rsio

nSt

ress

Gro

upResistor #4 T7

Resistor #4 T7



Details of R-Net #4 T7 after 105°C 24hr FoS

• Examination at 200x shows that the growth consists of a gray material with a metallic luster.

• Heavier growth is seen at the termination to metal interface.



Chip Resistor Findings• The FoS test method at 105C can induce silver sulfide

formation in silver conductor chip resistors.• Construction factors, such a coating overlap and

coating thickness, play a role in mitigation silver sulfide formation failure of silver conductor chip resistors.

• Process stresses, such as reflow and handling, must be considered in any part evaluation program. For example, SAC assembly induces higher stress on overcoat seam which may result in a higher potential for separation and silver sulfide failures.



Conclusions• The test methods discussed (Mixed Flowing Gas, Flowers of

Sulfur, and Clay Testing) all have strengths and weaknesses• Some conformal coat materials offer protection but other may

increase corrosion and poor coverage may also aggravated the situation

• Cover areas have been found to exhibit lower corrosion than exposed regions.

• Flower of Sulfur (FoS) test which was originated for porosity appears to be gaining favor for board and assembly tests.

• Product cleanliness and workmanship contribute to corrosion/electrochemical induced failures.

• Chip resistors with silver inner terminations are susceptible to sulfur based corrosion. Construction and assembly stresses are factors in dictating their susceptibility to corrosion.



For More Information on CALCE Research

http://www.calce.umd.edu/



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